食品安全质量检测学报
食品安全質量檢測學報
식품안전질량검측학보
FOOD SAFETY AND QUALITY DETECTION TECHNOLOGY
2013年
1期
82-88
,共7页
谢建军*%陈捷%李菊%袁震宇%谢玉珊
謝建軍*%陳捷%李菊%袁震宇%謝玉珊
사건군*%진첩%리국%원진우%사옥산
气相色谱/质谱法%QuEChERS%杀菌剂%残留测定
氣相色譜/質譜法%QuEChERS%殺菌劑%殘留測定
기상색보/질보법%QuEChERS%살균제%잔류측정
gas chromatography-mass spectrometry%QuEChERS%fungicides%residue detection
目的建立果蔬中20种杀菌剂(三环唑、五氯硝基苯、嘧霉胺、乙烯菌核利、百菌清、三唑酮、戊菌唑、腐霉利、三唑醇、多效唑、稻瘟灵、抑霉唑、咯菌腈、氟硅唑、腈菌唑、肟菌酯、丙环唑、咪鲜胺、腈苯唑、苯醚甲环唑)残留量的QuEChERS-GC/MS快速测定方法.方法以生菜、毛瓜、葡萄、李子为原料,样品经乙腈提取, PSA粉50.0 mg、Al2O3粉50.0 mg和NH2粉30.0 mg除杂净化后,用GC/MS外标法定量.结果三环唑等20种杀菌剂在0.025~0.250 mg/L的质量浓度范围内线性关系良好,相关系数为0.9974~1.0000.添加水平为0.05、0.1、0.2 mg/kg时,除百菌清外,其余19种杀菌剂平均回收率范围均处于83%~112%之间,相对标准偏差(RSD)小于11.0%,方法的检出限(LOD)为0.2~11.8μg/kg之间.结论本方法具有灵敏、快速、简便等特点,能满足果蔬中三环唑等20种农药杀菌剂的检测要求.
目的建立果蔬中20種殺菌劑(三環唑、五氯硝基苯、嘧黴胺、乙烯菌覈利、百菌清、三唑酮、戊菌唑、腐黴利、三唑醇、多效唑、稻瘟靈、抑黴唑、咯菌腈、氟硅唑、腈菌唑、肟菌酯、丙環唑、咪鮮胺、腈苯唑、苯醚甲環唑)殘留量的QuEChERS-GC/MS快速測定方法.方法以生菜、毛瓜、葡萄、李子為原料,樣品經乙腈提取, PSA粉50.0 mg、Al2O3粉50.0 mg和NH2粉30.0 mg除雜淨化後,用GC/MS外標法定量.結果三環唑等20種殺菌劑在0.025~0.250 mg/L的質量濃度範圍內線性關繫良好,相關繫數為0.9974~1.0000.添加水平為0.05、0.1、0.2 mg/kg時,除百菌清外,其餘19種殺菌劑平均迴收率範圍均處于83%~112%之間,相對標準偏差(RSD)小于11.0%,方法的檢齣限(LOD)為0.2~11.8μg/kg之間.結論本方法具有靈敏、快速、簡便等特點,能滿足果蔬中三環唑等20種農藥殺菌劑的檢測要求.
목적건립과소중20충살균제(삼배서、오록초기분、밀매알、을희균핵리、백균청、삼서동、무균서、부매리、삼서순、다효서、도온령、억매서、각균정、불규서、정균서、우균지、병배서、미선알、정분서、분미갑배서)잔류량적QuEChERS-GC/MS쾌속측정방법.방법이생채、모과、포도、리자위원료,양품경을정제취, PSA분50.0 mg、Al2O3분50.0 mg화NH2분30.0 mg제잡정화후,용GC/MS외표법정량.결과삼배서등20충살균제재0.025~0.250 mg/L적질량농도범위내선성관계량호,상관계수위0.9974~1.0000.첨가수평위0.05、0.1、0.2 mg/kg시,제백균청외,기여19충살균제평균회수솔범위균처우83%~112%지간,상대표준편차(RSD)소우11.0%,방법적검출한(LOD)위0.2~11.8μg/kg지간.결론본방법구유령민、쾌속、간편등특점,능만족과소중삼배서등20충농약살균제적검측요구.
Objective To develop a QuEChERS method combined with gas chromatography mass spec-trometry (GC/MS) for the determination of 20 kinds of fungicide residues (tricyclazole, quintozene, pyrimetha-nil, vinclozolin, chlorothalonil, triadimefon, penconazole, procymidone, triadimenol, paclobutrazol, iso-prothiolane, imazalil, fludioxonil, flusilazole, myclobutanil, trifloxystrobin, propiconazol, prochloraz, fenbu-conazole and difenoconazole) in vegetables and fruits. Methods Twenty kinds of fungicides residues were extracted from the samples (lettuce, hairy squash, grape and plum) with acetonitrile, and then detected by GC/MS with external standard method after being cleaned up with three sorbents (PSA 50.0 mg, Al2O3 50.0 mg and NH2 30.0 mg). Results The method showed a good linearity over the range of 0.025~0.250 mg/L with correlation coefficients of 0.9974~1.0000. The recoveries of fungicides, except Chlorothalonil, were in the range of 83%~112%with the spiked levels of 0.05, 0.1 and 0.2 mg/kg into four vegetables and fruits matrixes, and the relative standard deviations (RSDs) were almost not more than 11.0%. The limits of detections (LODs) were in the range of 0.2~11.8μg/kg, respectively. Conclusion The method is sensitive, rapid and simple, and can be used for the determination of 20 kinds of fungicides residues in vegetables and fruits.